Preparation method of phenol polyoxyethylene phosphonate

A technology of phenol polyoxyethylene ether phosphate and polyoxyethylene ether phosphate, which is applied in the field of anionization of nonionic surfactants in organic chemistry, can solve problems such as deep color cannot meet the needs of chemical fiber work applications, and achieve Product stability, strong pertinence, and excellent performance

Active Publication Date: 2011-06-01
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The phenol polyoxyethylene ether phosphate product prepared by the above method is brownish red, because the color of the product is deep and cannot meet the needs of chemical fiber work applications

Method used

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  • Preparation method of phenol polyoxyethylene phosphonate
  • Preparation method of phenol polyoxyethylene phosphonate
  • Preparation method of phenol polyoxyethylene phosphonate

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preparation example Construction

[0021] The preparation method of phenol polyoxyethylene ether phosphate of the present invention, it takes phenoxyethanol as initiator, under the presence of alkali catalyst (KOH, NaOH or sodium methylate any one or more than one mixture) and ring Ethylene oxide is polymerized to obtain phenol polyoxyethylene ether; the phenol polyoxyethylene ether is esterified with phosphorus pentoxide, and the target object of the esterification reaction is added to deionized water for hydrolysis, and the obtained phenol polyoxyethylene ether is Oxyethylene ether phosphate; the molar ratio of phenoxyethanol to ethylene oxide is 1:1-9; the molar ratio of phenol polyoxyethylene ether to phosphorus pentoxide is 2.0-3.5:1.

[0022] The added mass of the base catalyst is 0.1-1.5% of the mass sum of phenoxyethanol and ethylene oxide. The polymerization reaction temperature is 90-150° C., and the reaction time is 2-10 hours; the esterification reaction temperature is 60-90° C., and the reaction ti...

Embodiment 1

[0026] Add 275.0 g of phenoxyethanol and 1.0 g of KOH solid catalyst into a 2.5 L pressure reactor, and connect the ethylene oxide metering tank to the pressure tank. Replace the air with nitrogen for 3 times, wait until the temperature of the reaction kettle rises to 125-130°C, keep the system pressure at 0.2-0.3MPa, start to feed 789.1g of ethylene oxide, complete the passage in 3.0 hours, and continue the reaction for 7 hours. After the reaction was completed, it was cooled and the pressure was released to obtain 1064 grams (about 1.99 mol) of an intermediate whose main component was phenol polyoxyethylene ether phosphate. In the above steps, the molar ratio of phenoxyethanol to ethylene oxide is 1:9.

[0027] Transfer the obtained intermediate to a 1000mL four-neck flask, add 102.9g of phosphorus pentoxide in three batches, react at a temperature of 60-65°C for 10 hours, then add 11.7g of deionized water, and hydrolyze at a temperature of 70-75°C After cooling for 1.5 hou...

Embodiment 2

[0029] Add 150.0 g of phenoxyethanol and 7.3 g of sodium methoxide solid catalyst into a 2.5 L pressure reactor, and connect the ethylene oxide metering tank to the pressure reactor. Replace the air with nitrogen for 3 times, wait until the temperature of the reaction kettle rises to 90-95°C, keep the system pressure at 0.2-0.3MPa, start to feed 239.1g of ethylene oxide, complete the passage in 2.5 hours, and continue the reaction for 1.5 hours. After the reaction is complete, cool down and release the pressure. 489.1 g (about 1.09 mol) of an intermediate mainly composed of phenol polyoxyethylene ether phosphate was obtained. In the above steps, the molar ratio of phenoxyethanol to ethylene oxide is 1:5.

[0030] Transfer the obtained intermediate to a 1000mL four-neck flask, add 77.2g of phosphorus pentoxide in four batches, react at a temperature of 70-75°C for 4.5 hours, then add 9.3g of deionized water, and hydrolyze at a temperature of 85-90°C After cooling for 2.0 hour...

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Abstract

The invention discloses a preparation method of phenol polyoxyethylene phosphonate, comprising the following steps of: undergoing a polymerization reaction between epoxy ethane and phenoxyethanol as an initiator in the presence of a base catalyst to obtain phenol polyethenoxy ether; undergoing an esterification reaction between the phenol polyethenoxy ether and phosphorus pentoxide; and adding a target product of the esterification reaction into deionized water for hydrolyzing to prepare the phenol polyoxyethylene phosphonate, wherein the molar ratio of the phenoxyethanol to the epoxy ethane is 1:(1-9), and the molar ratio of the phenol polyethenoxy ether to the phosphorus pentoxide is (2.0-3.5):1. The base catalyst is one or a mixture of more of KOH, NaOH or NaOCH3. The invention has the advantages of reasonableness of raw material selection, determination of simple process and strong stability and pertinence of products. In addition, the final product provided by the invention is colourless.

Description

technical field [0001] The invention relates to a preparation method of phenol polyoxyethylene ether phosphate, which belongs to the technical field of anionization synthesis of nonionic surfactants in organic chemistry. Background technique [0002] At present, there are many reports on the synthesis of phenolic ether phosphates, which are generally prepared by reacting phenolic ethers with phosphorylating reagents. As phosphorylation reagents, phosphorus oxychloride, phosphorus pentoxide, etc. have been reported. Among them, the phosphorus pentoxide method is simple and easy, and the output is high, so it is the most commonly used method. However, because it is a strong oxidizing agent and a strong dehydrating agent, the product has different colors, especially as a chemical fiber oil agent, its color directly affects the quality of the fiber. Therefore, the synthesis of high-quality phenolic ethers is very important for controlling the color of phenolic ether phosphates....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/327C08G65/28C07F9/09D06M15/53D06M13/165
Inventor 王伟松王新荣曾红舟金一丰郭晓锋贾埂美
Owner ZHEJIANG HUANGMA TECH
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